CN102995083B - A kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array - Google Patents

A kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array Download PDF

Info

Publication number
CN102995083B
CN102995083B CN201210526589.XA CN201210526589A CN102995083B CN 102995083 B CN102995083 B CN 102995083B CN 201210526589 A CN201210526589 A CN 201210526589A CN 102995083 B CN102995083 B CN 102995083B
Authority
CN
China
Prior art keywords
array
nickel
nickel alloy
iron
alloy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201210526589.XA
Other languages
Chinese (zh)
Other versions
CN102995083A (en
Inventor
张海霞
李忠亮
孙旭明
郑阳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Peking University
Original Assignee
Peking University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Peking University filed Critical Peking University
Priority to CN201210526589.XA priority Critical patent/CN102995083B/en
Publication of CN102995083A publication Critical patent/CN102995083A/en
Application granted granted Critical
Publication of CN102995083B publication Critical patent/CN102995083B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Micromachines (AREA)

Abstract

It is an object of the invention to provide a kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array, the method adopts specific plating solution formula to reach the ratio of optimized alloy, thus realizing best soft magnet performance. The thin film of highly homogeneous 10 μm-50 μm can be grown in the Seed Layer of 0.15 μm. And it is simple to have technique, it is easy to accomplish, with low cost, be easy to the advantages such as Control release process. Plating solution formula from Row sum-equal matrix, can have great motility simultaneously. Carry out being easy to integrated with other technique after lithography. The array made is in the unit of 2000 μm * 2000 μm, it is simple to measure. By the manufacture method of array, the soft magnet performance of iron-nickel alloy material obtains great lifting. The magnetic of material is also had bigger lifting by the addition of nano magnetic granule simultaneously.

Description

A kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array
Technical field
The present invention relates to field of semiconductor manufacture, be specifically related to micro-nano processing technique field, particularly relate to a kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array.
Background technology
Iron-nickel alloy is a kind of material possessing good soft magnet performance, has narrow and thin hysteresis curve, remanent magnetization and coercivity all smaller, and initial permeability, up to more than 100000, has a wide range of applications in low-intensity magnetic field and RF application. Core material especially as MEMS inductance, it is possible to significant increase inductance value and quality factor (Q-value) so that inductance has good application under RF application.
MEMS (MEMS) is the technology of a kind of novel multi-crossed disciplines, and it relates to the multiple subjects such as machinery, electronics, chemistry, physics, optics, biology, material. In nanometer processing device, it is often necessary to process a kind of high performance magnetic material part of functions material as device, for instance the core material of MEMS inductance. In MEMS process technology, generally can passing through vacuum evaporation (evaporation), sputter (sputtering), methods such as (electroplating) of electroplating prepares alloy firm. Vacuum evaporation refers to heats thin-film material to be evaporated in a vacuum chamber so that it is atom or molecule, from surface gasification effusion, form steam and flow into the method penetrating and being deposited on solid (substrate).Sputtering is a kind of high-energy ion bombardment target, sputters atom or molecule deposition and forms the process of thin film on anode substrate. Such as, the Co-Femetal/native-oxidemultilayers:anewdirectioninsoftma gneticthinfilmdesignI.Quasi-staticpropertiesanddynamicre sponse(IEEEtransactiononMagnetics that G.S.D.Beach et al. delivered in 2005,2005.41 (6): p.2043--2052) (Chinese exercise question: ferro-cobalt and oxide layer multiple structure: the new direction of a soft magnetic film the quasi-static characteristics and dynamic response design) did the Slag coating technical study of CoFe alloy. And plating refers to and utilizes electrolysis principle method of the metal of some special component on some metal surface is electroplated. Compared to the advantage of first two method, electro-plating method is in that produced alloy internal stress is less, and manufacture process can control the alloy ratio of alloy firm by adjusting the composition of electroplate liquid, thus improving soft magnetic characteristic. Such as, the Microstructureandmagneticpropertiesinarraysofacelectrode positedFexNi1-xnanowiresinducedbythecontinuousandpulseel ectrodeposition that M.AlmasiKashi et al. delivered in 2011. (AppliedPhysicsA:MaterialsScience &Processing, 2011.102 (3): p.761--764) (Chinese exercise question: adopt the micro structure of iron-nickel alloy nano wire prepared by direct current and pulse current and the analysis of magnetic, International Periodicals: Applied Physics bulletin) did application alumina anode plating and prepare the experiment of ferrum nickel nano wire.
From described above it can be seen that electroplate a kind of method preparing alloy as maturation urgently study how to realize integrated processing among MEMS.
Summary of the invention
For the above-mentioned processing problems for iron-nickel alloy material, the present invention provides a kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array, and the method carries out the plating of specific alloy components containing by configuring specific electroplate liquid. Low stress, high performance soft magnetic film can be realized, and be prone to integrated with other micro-nano technology technical matters.
The present invention provides a kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array, comprises the steps: in order
Substrate sputter Seed Layer;
Thick resist lithography goes out array pattern;
Preparation electroplate liquid;
Power parameter is set, connects circuit;
Adjust electroplating time and uniform stirring equipment is electroplated;
Deluster photoresist with acetone;
Seed Layer is gone with glacial acetic acid and hydrogen peroxide;
It is annealed in vacuum chamber;
The soft magnet performance of test iron-nickel alloy array
In step (a), substrate is silicon chip, and Seed Layer is titanium copper Seed Layer, wherein titanium thickness 150Copper thickness 1500
In step (b), the design of array configuration displays figure and parameter designing, and array pattern includes circular array, quadrate array, rectangular array, monoblock is square and monoblock is circular, and photolithographic depth is 10-50 μm; Parameter designing includes the spacing between array sizes, array element, also has array pattern to account for the ratio of monoblock figure.
Step (c) prepares the composition of electroplate liquid and concentration includes: nickel sulfate NiSO4·6H2O:187g/L, Nickel dichloride. NiCl2·6H2O:50g/L, ferrous sulfate FeSO4·7H2O:64g/L, boric acid H3BO3: 40g/L, sodium chloride nacl: 20g/L, sodium lauryl sulphate NaC12H25SO4: 0.2g/L), phosphoric acid H3PO4: 5g/L, saccharin Saccharin:3.5g/L.
When ferrum nickel ratio is 7:93, only following two kinds of reagent need to be changed: nickel sulfate NiSO46H2O:176g/L, ferrous sulfate FeSO4·7H2O:18g/L。
When ferrum nickel ratio is 50:50, only following three kinds of reagent need to be changed: nickel sulfate NiSO4·6H2O:130.9g/L, Nickel dichloride. NiCl2·6H2O:35g/L, ferrous sulfate FeSO4·7H2O:179.2g/L。
Step (d) power parameter includes: electric current density, pulse frequency, dutycycle, electroplating time, power supply provides pulse current.
Step (c) mixes nano magnetic granule in electroplate liquid, to improve alloy soft magnetic performance.
Step (h) annealing temperature 600-700 DEG C, reduces internal stress by heat treatment process, promotes the homogeneity of alloy material.
The present invention provides a kind of iron-nickel alloy array, is make to prepare in aforementioned manners, and its thickness is 10-50 μm, and saturation induction density is more than 1T.
It is an object of the invention to provide the electro-plating method of a kind of reliable integrated iron-nickel alloy array, the method adopts specific plating solution formula to reach the ratio of optimized alloy, thus realizing best soft magnet performance. Homogeneity can be grown good, the thin film of highly homogeneous 10 μm-50 μm in the Seed Layer of 0.15 μm. And it is simple to have technique, it is easy to accomplish, with low cost, be easy to the advantages such as Control release process. Plating solution formula from Row sum-equal matrix, can have great motility simultaneously. Carry out being easy to integrated with other technique after lithography. The array made is in the unit of 2000 μm * 2000 μm, it is simple to measure. By the manufacture method of array, the soft magnet performance of iron-nickel alloy material obtains great lifting. The magnetic of material is also had bigger lifting by the addition of nano magnetic granule simultaneously.
Accompanying drawing explanation
By reading the detailed description that non-limiting example is made made with reference to the following drawings, the other features, objects and advantages of the present invention will become more apparent upon, and in accompanying drawing, same or analogous accompanying drawing labelling represents same or analogous parts.
Fig. 1 is that the present invention adopts plating to prepare the flow chart of steps of embodiment of the method for iron-nickel alloy array;
Fig. 2-Fig. 5 is the electron scanning micrograph of the iron-nickel alloy array surface using the method for the invention to prepare, wherein Fig. 2 is the plane graph of circular array, Fig. 3 is the plane graph of rectangular array, and Fig. 4 is the cross-sectional view of circular array, and Fig. 5 is the configuration of surface figure that amplification is bigger;
Fig. 6 is the equipment drawing of the electroplanting device that the present invention adopts;
Fig. 7 is the EDX composition analysis result of ferrum nickel (20:80) the alloy array using the method for the invention to prepare;
Fig. 8 is the EDX composition analysis result of ferrum nickel (7:93) the alloy array using the method for the invention to prepare;
Fig. 9 is the Magnetic Test result of ferrum nickel (20:80) alloy using the method for the invention to prepare;
Figure 10 is the Magnetic Test result of ferrum nickel (7:93) alloy using the method for the invention to prepare.
Detailed description of the invention
Understandable for enabling the above-mentioned purpose of the present invention, feature and advantage to become apparent from, below in conjunction with the drawings and specific embodiments, the embodiment of the present invention is described in further detail.
Being described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of same or like function from start to finish. The embodiment described below with reference to accompanying drawing is illustrative of, and is only used for explaining the present invention, and is not construed as limiting the claims.
Embodiment one:
It is a kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array of the present invention with reference to Fig. 1, Fig. 1, the flow chart of steps of embodiment, comprise the steps:
Step S1, adopts the method splash-proofing sputtering metal Ti150 of sputtering on the silicon chip in clean (110) crystal orientationNi metal 1500
Step S2, first drips photoresist at silicon chip surface, first carries out pre-spin coating 60s with the speed of 540r/s, then carries out the formal spin coating 180s of 1500r/s, it is ensured that photoresist is uniformly spreadable at silicon chip surface.Under litho machine, expose 125s, take out afterwards. Carry out drying film 210s at 80 DEG C. Then develop, developer solution soaks 120s. Guarantee development effect under the microscope.
Step S3, first the deionized water of measured amounts carries out the configuration of electroplate liquid. (introducing the configuration of electroplate liquid here for 1L). Pour deionized water into tank. Take appropriate medicine with projection electronic weighing and pour tank into. After all medicines are added by the electroplate liquid selecting ferrum nickel ratio to be 20:80, tank is put into 60 DEG C of water-baths, and uses Glass rod to be stirred helping reagent to dissolve. Candidate agent is completely dissolved, and uses PH reagent paper measure pH value and can pass through to add sodium hydroxide or sulphuric acid adjustment electroplate liquid pH value to 4.0.
Step S4, according to the area conversion source current size needing plating patterns on silicon chip, source current=electric current density * plating patterns area. The present invention adopts the electric current density of 4ASD, it is possible to be calculated needing the size of the source current of setting by plating patterns area. It is assumed here that be 80mA. Set dutycycle as 50%, forward conduction time 1ms, forward turn-off time 1ms, forward current 2ms, reverse current 0, thus set 0-80mA, dutycycle 50%, the pulse current of frequency 500Hz.
Step S5, circuit anode adopts clean nickel block, and negative electrode connects silicon chip. Silicon chip needs to clash the convenient conduction of electrode leads to client with acetone. Anode and cathode is put into connection power supply in electroplate liquid, checks that whether source current is correct. Pass into agitating device, make electroplate liquid in electroplating process keep uniformly. Set power supply ON time as 2h, switch on power and start plating.
Step S6, sets annealing temperature 670 DEG C, and annealing continues 2h. Cool down with the speed of 100 DEG C/h afterwards.
Step S7, is immersed in acetone soln by silicon chip 1min, treats that the photoresist on surface is all removed and takes out afterwards. Corrosive liquid is utilized (to remove Cu: glacial acetic acid, hydrogen peroxide and deionized water are according to the mixed liquor of the ratio of 1:1:20; Remove Ti: Fluohydric acid. and deionized water are according to the mixed liquor of the volume ratio of 1:60) remove Cu, Ti alloy Seed Layer of silicon chip surface. Silicon chip is fully cleaned in deionized water, and dries.
Step S8, utilizes scribing pen craft sliver, obtains sample. Sample is carried out the measurement of hysteresis curve.
With reference to the electron scanning micrograph (10 μm) that Fig. 2-Fig. 5, Fig. 2-Fig. 5 is the iron-nickel alloy array surface using the method for the invention to prepare. From photo it can be seen that plating alloy array out has good configuration of surface and homogeneity. Surface height difference is less than 0.5 μm. Fig. 2, Fig. 3 can be seen that array surface form and homogeneity are all relatively good, and the high multiple from Fig. 5 can be seen that under amplifying that homogeneity is very good, and as can be seen from Figure 4 the transverse section of array does not have slight crack flaw, and electroplating effect is good.
With reference to the EDX result figure that Fig. 7, Fig. 7 are iron-nickel alloy (20:80) array using the method for the invention to prepare. Result figure shows that iron-nickel alloy ratio is 20:80.
With reference to the Magnetic Test result that Fig. 9, Fig. 9 are iron-nickel alloy (20:80) prepared by the method for the invention on probation. From the shape of hysteresis curve and coordinate parameters it can be seen that sample presents good soft magnetic characteristic. Coercivity is relatively low, and for 1.345Oe, squareness ratio is 5.59*10-4, and saturation induction density can reach 1T.
Embodiment 2:
It is that the present invention adopts plating to prepare the flow chart of steps of embodiment of the method for iron-nickel alloy array with reference to Fig. 1, Fig. 1, comprises the steps:
Step S1, adopts the method splash-proofing sputtering metal Ti150 of sputtering on the silicon chip in clean (110) crystal orientationNi metal 1500
Step S2, first drips photoresist at silicon chip surface, first carries out pre-spin coating 60s with the speed of 540r/s, then carries out the formal spin coating 180s of 1500r/s, it is ensured that photoresist is uniformly spreadable at silicon chip surface.Under litho machine, expose 125s, take out afterwards. Carry out drying film 210s at 80 DEG C. Then develop, developer solution soaks 120s. Guarantee development effect under the microscope.
Step S3, first the deionized water of measured amounts carries out the configuration of electroplate liquid. (introducing the configuration of electroplate liquid here for 1L). Pour deionized water into tank. Take appropriate medicine with projection electronic weighing and pour tank into. After all medicines are added by the electroplate liquid selecting ferrum nickel ratio to be 7:93, tank is put into 60 DEG C of water-baths, and uses Glass rod to be stirred helping reagent to dissolve. Candidate agent is completely dissolved, and uses PH reagent paper measure pH value and can pass through to add sodium hydroxide or sulphuric acid adjustment electroplate liquid pH value to 4.0.
Step S4, according to the area conversion source current size needing plating patterns on silicon chip, source current=electric current density * plating patterns area. The present invention adopts the electric current density of 4ASD, it is possible to be calculated needing the size of the source current of setting by plating patterns area. It is assumed here that be 80mA. Set dutycycle as 50%, forward conduction time 1ms, forward turn-off time 1ms, forward current 2ms, reverse current 0, thus set 0-80mA, dutycycle 50%, the pulse current of frequency 500Hz.
Step S5, circuit anode adopts clean nickel block, and negative electrode connects silicon chip. Silicon chip needs to clash the convenient conduction of electrode leads to client with acetone. Anode and cathode is put into connection power supply in electroplate liquid, checks that whether source current is correct. Pass into agitating device, make electroplate liquid in electroplating process keep uniformly. Set power supply ON time as 2h, switch on power and start plating.
Step S6, sets annealing temperature 670 DEG C, and annealing continues 2h. Cool down with the speed of 100 DEG C/h afterwards.
Step S7, is immersed in acetone soln by silicon chip 1min, treats that the photoresist on surface is all removed and takes out afterwards. Corrosive liquid is utilized (to remove Cu: glacial acetic acid, hydrogen peroxide and deionized water are according to the mixed liquor of the ratio of 1:1:20; Remove Ti: Fluohydric acid. and deionized water are according to the mixed liquor of the volume ratio of 1:60) remove Cu, Ti alloy Seed Layer of silicon chip surface. Silicon chip is fully cleaned in deionized water, and dries.
Step S8, utilizes scribing pen craft sliver, obtains sample. Sample is carried out the measurement of hysteresis curve.
With reference to the electron scanning micrograph (10 μm) that Fig. 2-Fig. 5, Fig. 2-Fig. 5 is the iron-nickel alloy array surface using the method for the invention to prepare. From photo it can be seen that plating alloy array out has good configuration of surface and homogeneity. Surface height difference is less than 0.5 μm. Fig. 2, Fig. 3 can be seen that array surface form and homogeneity are all relatively good, and the high multiple from Fig. 5 can be seen that under amplifying that homogeneity is very good, and as can be seen from Figure 4 the transverse section of array does not have slight crack flaw, and electroplating effect is good.
With reference to the EDX result figure that Fig. 8, Fig. 8 are iron-nickel alloy (7:93) array using the method for the invention to prepare. Result figure shows that iron-nickel alloy ratio is 7:93.
With reference to the Magnetic Test result that Figure 10, Figure 10 are iron-nickel alloy (7:93) prepared by the method for the invention on probation. From the shape of hysteresis curve and coordinate parameters it can be seen that sample presents good soft magnetic characteristic. Coercivity is 29.13Oe, and squareness ratio is 0.13, and saturation induction density can reach 1.25T
Embodiment 3:
It is that the present invention adopts plating to prepare the flow chart of steps of embodiment of the method for iron-nickel alloy array with reference to Fig. 1, Fig. 1, comprises the steps:
Step S1, adopts the method splash-proofing sputtering metal Ti150 of sputtering on the silicon chip in clean (110) crystal orientationNi metal 1500
Step S2, first drips photoresist at silicon chip surface, first carries out pre-spin coating 60s with the speed of 540r/s, then carries out the formal spin coating 180s of 1500r/s, it is ensured that photoresist is uniformly spreadable at silicon chip surface.Under litho machine, expose 125s, take out afterwards. Carry out drying film 210s at 80 DEG C. Then develop, developer solution soaks 120s. Guarantee development effect under the microscope.
Step S3, first the deionized water of measured amounts carries out the configuration of electroplate liquid. (introducing the configuration of electroplate liquid here for 1L). Pour deionized water into tank. Take appropriate medicine with projection electronic weighing and pour tank into. After all medicines are added by the electroplate liquid selecting ferrum nickel ratio to be 20:80, tank is put into 60 DEG C of water-baths, and uses Glass rod to be stirred helping reagent to dissolve. Add magnetic nanoparticle Fe3O4, stir electroplate liquid. After candidate agent and magnetic nanoparticle are completely dissolved and are uniform, use PH reagent paper to measure pH value and also can pass through to add sodium hydroxide or sulphuric acid adjustment electroplate liquid pH value to 4.0.
Step S4, according to the area conversion source current size needing plating patterns on silicon chip, source current=electric current density * plating patterns area. The present invention adopts the electric current density of 4ASD, it is possible to be calculated needing the size of the source current of setting by plating patterns area. It is assumed here that be 80mA. Set dutycycle as 50%, forward conduction time 1ms, forward turn-off time 1ms, forward current 2ms, reverse current 0, thus set 0-80mA, dutycycle 50%, the pulse current of frequency 500Hz.
Step S5, circuit anode adopts clean nickel block, and negative electrode connects silicon chip. Silicon chip needs to clash the convenient conduction of electrode leads to client with acetone. Anode and cathode is put into connection power supply in electroplate liquid, checks that whether source current is correct. Pass into agitating device, make electroplate liquid in electroplating process keep uniformly. Set power supply ON time as 2h, switch on power and start plating.
Step S6, sets annealing temperature 670 DEG C, and annealing continues 2h. Cool down with the speed of 100 DEG C/h afterwards.
Step S7, is immersed in acetone soln by silicon chip 1min, treats that the photoresist on surface is all removed and takes out afterwards. Corrosive liquid is utilized (to remove Cu: glacial acetic acid, hydrogen peroxide and deionized water are according to the mixed liquor of the ratio of 1:1:20; Remove Ti: Fluohydric acid. and deionized water are according to the mixed liquor of the volume ratio of 1:60) remove Cu, Ti alloy Seed Layer of silicon chip surface. Silicon chip is fully cleaned in deionized water, and dries.
Step S8, utilizes scribing pen craft sliver, obtains sample. Sample is carried out the measurement of hysteresis curve.
With reference to the electron scanning micrograph (10 μm) that Fig. 2-Fig. 5, Fig. 2-Fig. 5 is the iron-nickel alloy array surface using the method for the invention to prepare. From photo it can be seen that plating alloy array out has good configuration of surface and homogeneity. Surface height difference is less than 0.5 μm. Fig. 2, Fig. 3 can be seen that array surface form and homogeneity are all relatively good, and the high multiple from Fig. 5 can be seen that under amplifying that homogeneity is very good, and as can be seen from Figure 4 the transverse section of array does not have slight crack flaw, and electroplating effect is good.
With reference to the EDX result figure that Fig. 7, Fig. 7 are the iron-nickel alloy array using the method for the invention to prepare. Result figure shows that iron-nickel alloy ratio is 20:80.
With reference to the Magnetic Test result that Fig. 9, Fig. 9 are iron-nickel alloy (20:80) prepared by the method for the invention on probation. From the shape of hysteresis curve and coordinate parameters it can be seen that sample presents good soft magnetic characteristic. Coercivity is relatively low, and for 1.345Oe, squareness ratio is 5.59*10-4, and saturation induction density can reach 1T.
Particular embodiments described above, has further described the purpose of the present invention, technical scheme and beneficial effect. It should be appreciated that above said content is only the specific embodiment of the present invention, it is not limited to the present invention. Within all essence in the present invention and ultimate principle, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Although being described in detail about example embodiment and advantage thereof, it should be understood that when the protection domain that spirit and the claims without departing from the present invention limit, it is possible to these embodiments are carried out various change, substitutions and modifications. For other examples, those of ordinary skill in the art is it should be readily appreciated that while keeping in scope, the order of processing step can change.
Additionally, the range of application of the present invention is not limited to the technique of the specific embodiment described in description, mechanism, manufacture, material composition, means, method and step. From the disclosure, will readily appreciate that as those of ordinary skill in the art, for having existed or be about to technique, mechanism, manufacture, material composition, means, method or the step developed at present later, wherein they perform the result that the function that is substantially the same of corresponding embodiment or acquisition with present invention description are substantially the same, and can they be applied according to the present invention. Therefore, claims of the present invention are intended to be included in its protection domain these technique, mechanism, manufacture, material composition, means, method or step.

Claims (10)

1. one kind adopts the method that soft magnetic materials iron-nickel alloy array is prepared in plating, it is characterised in that comprise the steps: in order
Sputtering seed layer in (a) substrate;
B () thick resist lithography goes out array pattern;
(c) preparation electroplate liquid;
D () arranges power parameter, connect circuit;
E () adjusts electroplating time and uniform stirring equipment is electroplated;
F () is delustered photoresist with acetone;
G () goes Seed Layer with glacial acetic acid and hydrogen peroxide;
H () is annealed in vacuum chamber;
The soft magnet performance of (i) test iron-nickel alloy array.
2. method according to claim 1, it is characterised in that:
In step (a), substrate is silicon chip, and Seed Layer is titanium copper Seed Layer, wherein titanium thicknessCopper thickness
3. method according to claim 1, it is characterised in that:
The array of designs figure of array configuration and parameter designing in step (b), array pattern includes circular array, quadrate array or rectangular array, and photolithographic depth is 10-50 μm; Parameter designing includes the spacing between array sizes, array element, and array pattern accounts for the ratio of monoblock figure.
4. method according to claim 1, it is characterised in that:
Step (c) prepares the composition of electroplate liquid and concentration includes: nickel sulfate NiSO4·6H2O:187g/L, Nickel dichloride. NiCl2·6H2O:50g/L, ferrous sulfate FeSO4·7H2O:64g/L, boric acid H3BO3: 40g/L, sodium chloride nacl: 20g/L, sodium lauryl sulphate NaC12H25SO4: 0.2g/L, phosphoric acid H3PO4: 5g/L, saccharin Saccharin:3.5g/L.
5. method according to claim 4, it is characterised in that:
When ferrum nickel ratio is 7:93, only following two kinds of reagent need to be changed: nickel sulfate NiSO4·6H2O:176g/L, ferrous sulfate FeSO4·7H2O:18g/L。
6. method according to claim 4, it is characterised in that:
When ferrum nickel ratio is 50:50, only following three kinds of reagent need to be changed: nickel sulfate NiSO4·6H2O:130.9g/L, Nickel dichloride. NiCl2·6H2O:35g/L, ferrous sulfate FeSO4·7H2O:179.2g/L。
7. method according to claim 1, it is characterised in that:
Step (d) power parameter includes: electric current density, pulse frequency, dutycycle, electroplating time, power supply provides pulse current.
8. method according to claim 1, it is characterised in that:
Step (c) mixes nano magnetic granule in electroplate liquid, to improve alloy soft magnetic performance.
9. method according to claim 1, it is characterised in that:
Step (h) annealing temperature 600-700 DEG C, reduces internal stress by heat treatment process, promotes the homogeneity of alloy material.
10. a soft magnetic materials iron-nickel alloy array, it is characterised in that: using the method for one of claim 1-9 to prepare, its thickness is 10-50 μm, and saturation induction density is more than 1T.
CN201210526589.XA 2012-12-07 2012-12-07 A kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array Active CN102995083B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210526589.XA CN102995083B (en) 2012-12-07 2012-12-07 A kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210526589.XA CN102995083B (en) 2012-12-07 2012-12-07 A kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array

Publications (2)

Publication Number Publication Date
CN102995083A CN102995083A (en) 2013-03-27
CN102995083B true CN102995083B (en) 2016-06-15

Family

ID=47924172

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210526589.XA Active CN102995083B (en) 2012-12-07 2012-12-07 A kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array

Country Status (1)

Country Link
CN (1) CN102995083B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103866364B (en) * 2014-03-06 2016-08-24 天津大学 The magnetospheric preparation method of stainless steel fibre Surface Fe nickel alloy
CN105780068B (en) * 2014-12-16 2018-02-02 北京有色金属研究总院 The method of single pulse electrodpositing Ni Fe alloy magnetic coating
CN108732863A (en) * 2018-05-24 2018-11-02 南方科技大学 A kind of flexible nano impression block and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020153255A1 (en) * 2001-04-20 2002-10-24 Dinan Thomas Edward Method of electroplating a nickel-iron alloy film with a graduated composition
WO2004094699A1 (en) * 2003-04-24 2004-11-04 Nano Invar Co. Ltd. Nano invar alloys and a process of producing the same
CN102723839A (en) * 2012-05-28 2012-10-10 北京大学 Electromagnetic energy harvester with flexible substrate and method for preparing electromagnetic energy harvester
CN102766893A (en) * 2012-07-24 2012-11-07 上海交通大学 Preparation method of nano porous copper capable of being patterned

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03291396A (en) * 1990-04-06 1991-12-20 Sumitomo Metal Ind Ltd Ni-fe alloy plating method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020153255A1 (en) * 2001-04-20 2002-10-24 Dinan Thomas Edward Method of electroplating a nickel-iron alloy film with a graduated composition
WO2004094699A1 (en) * 2003-04-24 2004-11-04 Nano Invar Co. Ltd. Nano invar alloys and a process of producing the same
CN102723839A (en) * 2012-05-28 2012-10-10 北京大学 Electromagnetic energy harvester with flexible substrate and method for preparing electromagnetic energy harvester
CN102766893A (en) * 2012-07-24 2012-11-07 上海交通大学 Preparation method of nano porous copper capable of being patterned

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Zhongliang Li等.Microstructure and magnetic properties of micro NiFe alloy arrays for MEMS application.《J. Micromech. Microeng.》.2013,第23卷(第8期),第1-8页. *
杨锋等.电沉积铁镍合金薄膜及其结构与磁性能的研究.《表面技术》.2012,第41卷(第2期),第1节实验. *
陈闪闪等.电沉积纳米晶Ni–Fe 合金在碱性溶液中的腐蚀性能.《中国表面工程》.2008,第21卷(第5期),第54-58页. *

Also Published As

Publication number Publication date
CN102995083A (en) 2013-03-27

Similar Documents

Publication Publication Date Title
Yoo et al. Electrodeposition of FeCoNi thin films for magnetic-MEMS devices
Park et al. Nanostructured magnetic CoNiP electrodeposits: Structure–property relationships
Bertero et al. Electrodeposition of amorphous Fe-Cr-Ni stainless steel alloy with high corrosion resistance, low cytotoxicity and soft magnetic properties
Su et al. Influence of pH and bath composition on properties of Ni–Fe alloy films synthesized by electrodeposition
JP2010515820A (en) Formation of nanostructures containing compositionally modulated ferromagnetic layers by pulsed ECD
CN102995083B (en) A kind of method adopting plating to prepare soft magnetic materials iron-nickel alloy array
Fesharaki et al. Magnetoresistance and structural study of electrodeposited Ni-Cu/Cu multilayers
CN102400191B (en) Method for preparing Sm-Fe (samarium-ferrum) alloy magnetic thin film under intense magnetic field
Guan et al. Pulse-reverse electrodeposited nanograinsized CoNiP thin films and microarrays for MEMS actuators
Mardani et al. Electrodeposition of Ni32Fe48Mo20 and Ni52Fe33W15 alloy film on Cu microwire from ionic liquid containing plating bath
CN105780068A (en) Single-pulse electrodeposition method for Ni-Fe alloy magnetic coatings
Varea et al. Ordered arrays of ferromagnetic, compositionally graded Cu 1− x Ni x alloy nanopillars prepared by template-assisted electrodeposition
Sanz-Hernández et al. Nanofabrication of three-dimensional magnetic structures
Zeng et al. Gradient magnetic binary alloy nanowire
Bodea et al. Electrochemical growth of iron and cobalt arborescences under a magnetic field
Myung et al. Electrodeposition of Ni/Cu multilayers
Li et al. Effect of boron/phosphorus-containing additives on electrodeposited CoNiFe soft magnetic thin films
Wang et al. Optimum electrodeposition conditions of FeCoZr films with in-plane uniaxial anisotropy for high frequency application
Chouarbi et al. SmCo micromolding in an aqueous electrolyte
Saraç et al. The effect of boric acid content on the properties of electrochemically prepared Ni-Fe/ITO thin films.
Rani et al. Characterization of Electroplated Permalloy Film on Microstructure for Bio-MEMS Application
Medouer et al. A Study of the Optimal Composition of the Bath Used for the Electrodeposition of Invar Alloy Thin Films
Xiao et al. Preparation and Magnetic Properties of Fe-Co–Ni Magnetic Nanowire Arrays with Three-Dimensional Periodic Structures
Lv et al. Design and fabrication of low power consumption micro fluxgate sensor
Saraç et al. Improvement of some physical and magnetic properties of nanocrystalline Fe15–Ni85/ITO thin films by galvanostatic pretreatment process

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant